CN102327214A - Thymol nano-medicament and preparation method thereof - Google Patents
Thymol nano-medicament and preparation method thereof Download PDFInfo
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- CN102327214A CN102327214A CN201110243511A CN201110243511A CN102327214A CN 102327214 A CN102327214 A CN 102327214A CN 201110243511 A CN201110243511 A CN 201110243511A CN 201110243511 A CN201110243511 A CN 201110243511A CN 102327214 A CN102327214 A CN 102327214A
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Abstract
The invention discloses a thymol nano-medicament, which is prepared from the following raw materials in percentage by mass: 0.1-5 percent of thymol, 0.1-5 percent of oil phase, 20-40 percent of surfactant, 4-20 percent of cosurfactant and the balance of distilled water, wherein the total mass percentage of the raw materials is 100 percent. The thymol nano-medicament has the advantages of high thermodynamic stability, high storage stability, non-delamination by long-time standing, high liquid drop dispersion degree and high bioavailability, and can be used for safely and effectively treating dermatozoiasis.
Description
Technical field
The invention belongs to field of medicaments, relate to a kind of miticide novel form, particularly a kind of method for preparing of thymol Nano medication of stable transparent.
Background technology
Thymol (thymol) has another name called thymol; Be a kind of monoterpene phenol; Being the derivant of p-Cymene, being mainly derived from the Thymus plant, is the Herba thymi vulgaris main component of essential oil; Have antibacterial widely, anticorrosion, antioxidation, antiinflammatory, eliminate the phlegm, the acaricide isoreactivity, find also that in recent years it has obvious antineoplastic.Thymol room temperature down for white to light yellow crystalline powder, be slightly soluble in water, be soluble in organic solvent, its character is extremely unstable in the production of conventional dosage forms and storage, is prone to lost and influences drug effect.Mostly the medicine of treating the skin acaricide in the market is ivermectin, and its life cycle is longer, bigger for the zootoxin side effect, and effect is not remarkable.
Summary of the invention
To the shortcomings and deficiencies that exist in the prior art, the present invention processes nano-emulsion to thymol, has strengthened the effectiveness of thymol greatly, has also solved thymol simultaneously and has been insoluble in water, shortcomings such as poor stability.
Because nano-emulsion substrate belongs to the nanoscale emulsion; It can make medicine be dissolved in the emulsion droplet; And improve stability of drug and percutaneous permeability and medicine bioavailability, so the present invention is solubilized into thymol in the nano-emulsion substrate, processes the external preparation for skin medicine; For veterinary clinic provides a kind of new acaricide medicine, thereby animal parasitosis is played treatment and preventive effect.
The technical method of realizing the foregoing invention purpose is the thymol nano-emulsion, and it is made up of the following weight proportion raw material:
Thymol 0.1%～5%, oil phase 0.1%～5%, surfactant are 20%～40%, cosurfactant is 4%～20%, surplus is a distilled water, and the mass percent sum of above-mentioned raw materials is 100%.
The formula optimization mass percent scope for preparing thymol Nano medication of the present invention is: thymol 0.5%～2.5%, oil phase 0.5%～4%, surfactant are 25%～35%, cosurfactant is 4.5%～10%, surplus is a distilled water, and the mass percent sum of above-mentioned raw materials is 100%.
The prescription best in quality percentage ratio for preparing thymol Nano medication of the present invention is: thymol 1%, oil phase 2%, surfactant are 27%, cosurfactant is 9%, distilled water 61%.
Described surfactant is one or more the mixture in Tween-60 (Tween-60), tween 80 (Tween-80), tween 20 (Tween-20), polyoxyethylene (40) Oleum Ricini (EL-40), polyoxyethylene (40) castor oil hydrogenated (RH-40) and the Arlacel-80 (Span-80).
Described cosurfactant is a dehydrated alcohol, 1, the mixture of one or more in 2-propylene glycol, ethylene glycol, glycerin, Macrogol 200 (PEG 200), PEG400 (PEG 400), the Macrogol 600 (PEG 600).
Described oils and fats is one or more the mixture in ethyl acetate, oleic acid, triacetyl glycerine, ethyl oleate, glycerin methylal, isopropyl myristate, vitamin E oil, liquid paraffin, almond oil, Jojoba oil, olive oil, Oleum Ricini, the Semen Tritici aestivi germ oil.
On surfactant selection, the present invention selects the nonionic surfactant of avirulence and good biocompatibility for use.Nonionic surfactant is more stable in solution, is not subject to the influence of strong electrolyte, inorganic salts, also is not subject to the influence of soda acid, and good with the compatibility of other surfactants, haemolysis is less.In theory; The HLB value that the preparation of O/W type nanometer emulsion needs surfactant is between 8～18; Consider preparation technology's simplicity; Be the easy formation property of nano-emulsion and the stability of nano-emulsion, the present invention selects the liquid nonionic surfactant of HLB between 10～15 for use, and is perhaps composite with the nonionic surfactant of a kind of HLB＜10.Available surfactant has: the mixture of one or more among Tween-60, Tween-80, Tween-20, EL-40, RH-40 and the Span-80.
The present invention is according to when the HLB value of the required surfactant of emulsifying oil phase is close with surfactant; The principle that formed emulsion is stable, the oils and fats of selecting for use has: the mixture of one or more in ethyl acetate, oleic acid, triacetyl glycerine, ethyl oleate, glycerin methylal, isopropyl myristate, vitamin E oil, liquid paraffin, almond oil, Jojoba oil, olive oil, Oleum Ricini, the Semen Tritici aestivi germ oil.The formation of most of nano-emulsion all need add cosurfactant, and its effect mainly contains: reduce interfacial tension between profit, the flowability that increases interfacial film, the HLB value of reconciliation statement surface-active agent etc.The cosurfactant that the present invention selects for use has dehydrated alcohol, 1, the mixture of one or more among 2-propylene glycol, ethylene glycol, glycerin, PEG 200, PEG 400, the PEG 600.
The present invention goes back the method for preparing that a purpose provides above-mentioned thymol Nano medication, it is characterized in that, specifically comprises the following steps:
1) take by weighing thymol, oil phase, surfactant, cosurfactant, distilled water, subsequent use;
2) thymol is added in the oil phase, stir;
3) with step 2) solution of preparation adds to stir in the cosurfactant that it is dissolved fully, surfactant is added wherein again, stir;
4) solution with the step 3) preparation fully stirs at 20 ℃～25 ℃ slow down adding distilled water, has mobile yellow or water white thymol Nano medication for a short time until formation clear, viscosity.
Thymol Nano medication of the present invention has the function of treatment skin acaricide.Usage: be coated with every day 1～2 time, continuous 1～2 week outside local.
The present invention detects through transmission electron microscope, and droplet diameter distribution is between 1～100nm, and outward appearance is yellow or colourless transparent liquid, has good stability:
1. light stability
Thymol Nano medication of the present invention is packed in the vial, and sealing places room temperature, and illumination 10d is in 1d, 3d, 5d, 7d, the 10d detection of taking a sample.The result shows that thymol Nano medication outward appearance of the present invention is clear still, does not have phenomenons such as muddiness, layering, deposition, and particle diameter remains between 1nm ~ 100nm.
2. temperature stability
An amount of thymol Nano medication of the present invention is packed in the vial, and sealing places 4 ℃ respectively, 25 ℃ with 37 ℃ of three kinds of temperature conditions under keep sample and investigate 30d, every at a distance from 5d sampling observation.The result shows that thymol Nano medication of the present invention all keeps clear under these three kinds of temperature conditions, do not see layering, muddiness and sedimentary phenomenon.
3. anti-freeze-stable property
Thymol Nano medication of the present invention in-4 ℃ of one weeks of preservation, is returned to room temperature after the taking-up.Thymol Nano medication of the present invention becomes solid in the time of-4 ℃, return to after the room temperature it and return to transparently, and places after a week still clear.
4. accelerated stability
Thymol Nano medication of the present invention is placed centrifuge tube, and in the centrifugal 20min of 15000rpm, observed result is found its not layering, still clear.
Thymol Nano medication of the present invention compared with prior art has the following advantages:
1) thermodynamic stability is good, and bin stability is high, put for a long time not stratified, through centrifugal acceleration test layering not yet;
2) the invention belongs to nano-grade medicine, the outward appearance clear, the emulsion droplet dispersion is good, and bioavailability is high;
3) medicine of the present invention can be treated dermatozoiasis safely and effectively.
4) preparation technology is simple, is fit to large-scale production.
Description of drawings
Fig. 1 is the transmission electron microscope picture of thymol Nano medication of the present invention.
Fig. 2 is the particle size distribution figure of thymol Nano medication of the present invention.
The specific embodiment
Below further set forth the beneficial effect that the present invention narrates medicine through Test Example, these Test Example comprise medicine of the present invention transmission electron microscope observation test, sizing assay test, exsomatize and kill demodicid mite test and clinical efficacy test.
Test Example 1Thymol Nano medication transmission electron microscopy observation of the present invention
Medicine of the present invention carries out microscopic pattern with transmission electron microscope to be observed; Fig. 1 is seen in result's demonstration; Fig. 1 is thymol nano-emulsion transmission electron microscope photo (* 50 000), show that thymol Nano medication drop is spherical in shape and be evenly distributed, decentralized is good, particle diameter is all less than 100nm.
Test Example 2The results of grain size analysis of thymol Nano medication of the present invention
Medicine of the present invention carries out grain size analysis with Particle Size Analyzer; The result sees Fig. 2; Fig. 2 is the particle size distribution figure of thymol nano-emulsion, and the mean diameter of thymol Nano medication (Z – Average) is 16.4 nm, and polydispersity coefficient (PDI) is 0.062; Its particle size distribution range is narrower, and particle diameter is all in 100 nm.
Test Example 3The demodicid mite test is killed in exsomatizing of thymol Nano medication of the present invention
Scrape the crust and the epidermis affected part scurf that cover with blood crusts in the rabbit auditory meatus of taking from right infection acarid, and place in the glass dish with the tweezers taking-up, the plate edge is coated with a small amount of acarid repellent agent, heats a little, is for experiment with choosing the active strong acarid of worm pin picking.
With separating pin picking acarid on the spill microscope slide; Drip and supply two of reagents, 8 of the acarids of selecting are placed medicinal liquid and add coverslip, under inverted microscope, continue to observe 24h; Every separated 5min observes once; Each observation 2min that continues observes until all death of 8 acarids, record acarid death time every group.It is 3 groups that test is divided into, and all the other two groups is distilled water test group and ivermectin injection group, and test method is with thymol Nano medication group of the present invention.
Result of the test: different medicinal liquids are handled 24h result and are shown that it is 3min that the thymol Nano medication kills the demodicid mite time, is lower than the ivermectin injection group, and its miticidal effect is better than ivermectin injection.The result sees table 1.
The table 1 miticidal effect comparative result that exsomatizes
Annotate :+expression has the acarid survival;-expression acarid all kills does not have recovery
Test Example 4The clinical efficacy test of thymol Nano medication of the present invention
At hospital admission, make a definite diagnosis the sick acaricide of trouble skin through check; After obtaining owner and agreeing, meet several 40 of the house pet of this experimental condition, as this object of study.Trial drug directly is applied to the affected part, and 14 d, are used continuously at every day twice in cleaning and dry affected part before the medication.The observed and recorded result of the test.
The effective percentage of table 2 medicine
The clinical efficacy result of the test shows; Thymol Nano medication effective percentage is 95%; And the effective percentage of clinical commonly used drug ivermectin is 90%, explains that the clinical therapeutic efficacy of thymol Nano medication is superior to ivermectin, and safety; Untoward reaction is few, has broad prospect of application aspect the treatment of skin acaricide.
Below the embodiment that provides through the inventor method for preparing of coming further to set forth thymol Nano medication of the present invention.
Embodiment 1
1) take by weighing thymol 0.1g, 0.1g, 3g, 0.5g, distilled water 6.3g, subsequent use;
2) thymol is added in the ethyl oleate, stir;
3) with step 2) solution of preparation adds to stir in the dehydrated alcohol that it is dissolved fully, EL-40 is added wherein again, stir;
4) solution with the step 3) preparation fully stirs at 20 ℃～25 ℃ slow down adding distilled water, has mobile yellow or water white thymol Nano medication for a short time until formation clear, viscosity.
Embodiment 2
Thymol 0.2g, isopropyl myristate 0.02g, ethyl acetate 0.02g, RH-40 3g, dehydrated alcohol 0.5g, 1,2-propylene glycol 0.3g, distilled water 5.96g.
Embodiment 3
Thymol 0.5g, olive oil 0.05g, isopropyl myristate 0.05g, Tween-80 3.5g, Tween-60 0.5g, dehydrated alcohol 0.5g, ethylene glycol 0.5g, distilled water 4.4g.
Embodiment 4
Thymol 0.05g, Jojoba oil 0.1g, almond oil 0.1g, Tween-80 3g, Tween-20 0.5g, dehydrated alcohol 0.25g, ethylene glycol 0.25g, distilled water 5.75g.
Embodiment 5
Thymol 0.2g, ethyl acetate 0.1g, EL-40 3g, dehydrated alcohol 0.5g, distilled water 6.2g.
Embodiment 6
Thymol 0.01g, ethyl acetate 0.5g, Tween-80 3.5g, dehydrated alcohol 0.4g, PEG400 0.1g, distilled water 5.49g.
Embodiment 7
Thymol 0.05g, Semen Tritici aestivi germ oil 0.05g, liquid paraffin 0.05g, RH-40 2g, dehydrated alcohol 0.8g, distilled water 7.05g.
Embodiment 8
Thymol 0.1g, vitamin E oil 0.1 g, oleic acid 0.1 g, Tween-80 3g, dehydrated alcohol 2g, distilled water 4.7g.
Embodiment 9
Thymol 0.1g, isopropyl myristate 0.1g, Tween-80 3g, Span-80 0.5g, PEG600 0.25g, PEG200 0.25g, distilled water 5.8g.
Thymol 0.3g, glycerin methylal 0.01g, glyceryl triacetate 0.01g, Tween-80 3g, dehydrated alcohol 0.4g, distilled water 6.28g.
Claims (9)
1. thymol Nano medication; It is characterized in that; The particle diameter of this medicine is 1nm～100nm; Raw material by following mass percent is processed: thymol 0.1%～5%, oil phase 0.1%～5%, surfactant are 20%～40%, cosurfactant 4%～20%, surplus are distilled water, and the mass percent sum of mentioned component is 100%;
Described surfactant is one or more the mixture among Tween-60, Tween-80, Tween-20, EL-40, RH-40 and the Span-80;
Described cosurfactant is a dehydrated alcohol, 1, the mixture of one or more among 2-propylene glycol, ethylene glycol, glycerin, PEG 200, PEG 400, the PEG 600;
Described oil phase is one or more the mixture in ethyl acetate, oleic acid, triacetyl glycerine, ethyl oleate, glycerin methylal, isopropyl myristate, vitamin E oil, liquid paraffin, almond oil, Jojoba oil, olive oil, Oleum Ricini, the Semen Tritici aestivi germ oil.
2. thymol Nano medication according to claim 1; It is characterized in that; Raw material by following mass percent is processed: thymol 0.5%～2.5%, oil phase 0.5%～4%, surfactant are 25%～35%, cosurfactant is 4.5%～10%, surplus is a distilled water, and the mass percent sum of above-mentioned raw materials is 100%.
3. a thymol Nano medication is characterized in that, is processed by the raw material of following mass percent: thymol 1%, oil phase 2%, surfactant are 27%, cosurfactant is 9%, distilled water 61%.
4. a thymol Nano medication is characterized in that, is processed by the raw material of following mass percent: thymol 1%, ethyl oleate 1%, EL-40 30%, dehydrated alcohol 5%, distilled water 63%.
5. a thymol Nano medication is characterized in that, is processed by the raw material of following mass percent: thymol 2%, isopropyl myristate 0.2%, ethyl acetate 0.2%, RH-40 30%, dehydrated alcohol 5%, 1,2-propylene glycol 3%, distilled water 59.6%.
6. thymol Nano medication; It is characterized in that, process: thymol 0.5%, Jojoba oil 1%, almond oil 1%, Tween-80 30%, Tween-20 5%, dehydrated alcohol 2.5%, ethylene glycol 2.5%, distilled water 57.5% by the raw material of following mass percent.
7. a thymol Nano medication is characterized in that, is processed by the raw material of following mass percent: thymol 2%, ethyl acetate 1%, EL-40 30%, dehydrated alcohol 5%, distilled water 62%.
8. a thymol Nano medication is characterized in that, by being processed by the raw material of following mass percent: thymol 1%, isopropyl myristate 1%, Tween-80 30%, Span-80 5%, PEG600 2.5%, PEG200 2.5%, distilled water 58%.
9. the method for preparing of the said thymol Nano medication of claim 1 is characterized in that, specifically comprises the following steps:
1) take by weighing thymol, oil phase, surfactant, cosurfactant, distilled water, subsequent use;
2) thymol is added in the oil phase, stir;
3) with step 2) solution of preparation adds to stir in the cosurfactant that it is dissolved fully, surfactant is added wherein again, stir;
4) solution with the step 3) preparation fully stirs at 20 ℃～25 ℃ slow down adding distilled water, has mobile yellow or water white thymol Nano medication for a short time until formation clear, viscosity.
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Cited By (9)
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| CN105123990A (en) * | 2015-10-08 | 2015-12-09 | 河南工业大学 | Method for preparing stable type sesamol microemulsion |
| CN107197860A (en) * | 2016-03-17 | 2017-09-26 | 新加坡国立大学 | Nano-emulsion containing carvacrol and preparation method thereof |
| CN107550862A (en) * | 2017-09-15 | 2018-01-09 | 成都泠汐尚品科技有限公司 | A kind of Thymol nano-emulsion and preparation method thereof |
| CN108013029A (en) * | 2017-12-29 | 2018-05-11 | 咸阳职业技术学院 | A kind of compound phenol nanoemulsion and its preparation method and application |
| CN108719457A (en) * | 2018-05-31 | 2018-11-02 | 武汉轻工大学 | Nanoemulsions and its preparation method and application with bacteriostatic activity thymol |
| CN108743950A (en) * | 2018-06-29 | 2018-11-06 | 佛山市南海东方澳龙制药有限公司 | Insecticide and preparation method thereof |
| CN109999014A (en) * | 2019-03-28 | 2019-07-12 | 佛山市正典生物技术有限公司 | It is a kind of can the new merit chigger disease of prevention and control plants essential oil and preparation method thereof |
| CN113632797A (en) * | 2021-08-30 | 2021-11-12 | 广西壮族自治区亚热带作物研究所（广西亚热带农产品加工研究所） | Synergistic composition for preventing and treating papaya mites |
| CN115737559A (en) * | 2022-12-06 | 2023-03-07 | 西北农林科技大学 | Oil-in-water type nervonic acid nanoemulsion and preparation method and application thereof |
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| CN105123990A (en) * | 2015-10-08 | 2015-12-09 | 河南工业大学 | Method for preparing stable type sesamol microemulsion |
| CN105123990B (en) * | 2015-10-08 | 2021-08-06 | 河南工业大学 | Method for preparing stable sesamol microemulsion |
| CN107197860A (en) * | 2016-03-17 | 2017-09-26 | 新加坡国立大学 | Nano-emulsion containing carvacrol and preparation method thereof |
| CN107197860B (en) * | 2016-03-17 | 2021-12-07 | 新加坡国立大学 | Nanometer emulsion containing carvacrol and preparation method thereof |
| CN107550862A (en) * | 2017-09-15 | 2018-01-09 | 成都泠汐尚品科技有限公司 | A kind of Thymol nano-emulsion and preparation method thereof |
| CN108013029A (en) * | 2017-12-29 | 2018-05-11 | 咸阳职业技术学院 | A kind of compound phenol nanoemulsion and its preparation method and application |
| CN108719457A (en) * | 2018-05-31 | 2018-11-02 | 武汉轻工大学 | Nanoemulsions and its preparation method and application with bacteriostatic activity thymol |
| CN108743950A (en) * | 2018-06-29 | 2018-11-06 | 佛山市南海东方澳龙制药有限公司 | Insecticide and preparation method thereof |
| CN109999014A (en) * | 2019-03-28 | 2019-07-12 | 佛山市正典生物技术有限公司 | It is a kind of can the new merit chigger disease of prevention and control plants essential oil and preparation method thereof |
| CN113632797A (en) * | 2021-08-30 | 2021-11-12 | 广西壮族自治区亚热带作物研究所（广西亚热带农产品加工研究所） | Synergistic composition for preventing and treating papaya mites |
| CN115737559A (en) * | 2022-12-06 | 2023-03-07 | 西北农林科技大学 | Oil-in-water type nervonic acid nanoemulsion and preparation method and application thereof |
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Application publication date: 20120125 |